CN1117139C - Dewatering tech. for microwater in organic solvent - Google Patents
Dewatering tech. for microwater in organic solvent Download PDFInfo
- Publication number
- CN1117139C CN1117139C CN 97126199 CN97126199A CN1117139C CN 1117139 C CN1117139 C CN 1117139C CN 97126199 CN97126199 CN 97126199 CN 97126199 A CN97126199 A CN 97126199A CN 1117139 C CN1117139 C CN 1117139C
- Authority
- CN
- China
- Prior art keywords
- tower
- air
- organic solvent
- water
- sorbent material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention discloses a dewatering technology for trace water in organic solvents, which is characterized in that the dewatering technology comprises the following procedures: (1) making organic solvents pass through adsorbing agents in a fixed bed filled tower; (2) draining out solutions stored in the tower when the adsorbing agents approach saturation as a result of absorbing water, carrying out vacuum dewatering, and then blowing the tower by dry air until the concentration of flammable gas in gas at a tower outlet is beyond explosion limits; (3) regenerating the adsorbing agents under normal pressure by heat dry air; and (4) cooling the towel to normal temperature by dry cold air. The procedures are carried out repeatedly. The technology has the advantages of simple technical process, convenient operation, low dehydration depth of organic solvents, repeated use of molecular sieves and prolonged service life of molecular sieves.
Description
The present invention relates to the dewatering of solvent, the absorbing process that removes of minor amount of water in a kind of organic solvent is provided especially.
Document related to the present invention is not reported at present.The patent documentation overwhelming majority of publishing is the dewatering of specific a certain solution.As " removing the absorbing process of water and methyl alcohol in the alcohol " of inventions such as Sun Weiruo, Chinese patent, publication number CN 1036944A.This invention is at water in the alcohol and methyl alcohol, its core is to use earlier the corn adsorption tower, the back removes moisture content and methyl alcohol in the alcohol with the zeolite molecular sieve adsorption tower, can make the alcohol of 90% (V) remove moisture content, methyl alcohol and some other impurity obtain the alcohol of 95.5% (V) or 99.6% (V), below its methanol content 200ppm.This method need consume a large amount of nitrogen or carbon monoxide gas when adsorbent reactivation, its dehydration degree of depth is dark inadequately, can not get the straight alcohol of water content ppm level, inconvenient operation, and because of the corn tower easily blocks, the facility investment amount is bigger.In addition, U.S.'s union carbide corporation John Draenor is thanked to Germania etc. and has been invented " adopting the drying means of Chabazite-type sorbent material ", Chinese patent, CN 86208824A, this method is at the acidic fluid that contains moisture content and at least a acidic cpd, is applicable to the drying of gas.Sorbent material is the Chabazite-type zeolite.This method is better to following sour gas effect: halohydrocarbon, alcohol, ether, organic acid, ketone etc.Well-known in the prior art, when organic solvent adopted the sorbent material dehydration, solvent should fully contact with sorbent material.Its principle is that the water molecules diameter is less, molecular sieve is a porous mass, when molecular sieve bore diameter during greater than the water molecules diameter and less than the molecular dimension of organic solvent, the organic solvent molecule can be stayed beyond the adsorbent surface in theory, water molecules then is adsorbed to inner surface, sorbent material duct, can reach the purpose of dehydration like this.When sorbent material suction when saturated, reproducing adsorbent recycles.Such dewatering can not make water and sorbent material generation chemical reaction generate hydrate, belongs to the physical adsorption dewatering.Except that molecular sieve, silica gel, gac also can be used as sorbent material.Another kind of is the chemisorption dewatering, as being sorbent material with calcium sulfate, calcium chloride, peroxophosphoric acid magnesium etc., by water and their water generation reaction compounds.In general, the physical adsorption dehydration is made the sorbent material best results with molecular sieve.But the intensity of molecular sieve and age limit it in industrial application.
The object of the present invention is to provide the removing process of minor amount of water in a kind of organic solvent, it can be implemented in the minor amount of water that industrial use molecular sieve adsorption removes organic solvent, its technical process is simple, easy to operate, can make the dehydration of organic solvent degree of depth low, and molecular sieve can use repeatedly, has prolonged molecular sieve work-ing life.
The invention provides the removing process of minor amount of water in a kind of organic solvent, it is characterized in that operating process is as follows:
(1) water smoking
Make organic solvent with the void tower linear speed of 0.5～20cm/min by the sorbent material in the fixed bed packing tower, the aspect ratio 5～30 of tower, organic solvent fully contacts with sorbent material, 1～24 hour duration of contact, the initial water content of organic solvent should be less than 1%;
(2) purge stages of residual solvent in the tower
When sorbent material suction when saturated, storing liquid in tower is put only, vacuum desorption 1～5 hour purged 2～10 hours with dry air then, inflammable gas concentration is beyond limits of explosion in tower is worked off one's feeling vent one's spleen, air moisture content requirement dew point is lower than-20 ℃;
(3) the adsorbent reactivation stage
Be used for warm air sorbent material is regenerated under normal pressure, 200～500 ℃ of temperature, 2～24 hours time, air moisture content requires dew point to be lower than-20 ℃, regeneration tolerance 0.8～3.0NM
3/ hrKg molecular sieve;
(4) sorbent material temperature-fall period
Be used for freezing air temperature in the tower is reduced to normal temperature, air moisture content requires dew point to be lower than-20 ℃.
Above-mentioned steps repeats.
In addition, organic solvent of the present invention comprises aromatic hydrocarbons, alkanes, alcohols, amides, alkyl halide class etc.Sorbent material comprises A type, X type, Y type, mordenite type, ZSM type, MCM series molecular sieve.
Above-mentioned dehydration tower aspect ratio is preferably 10～15, and organic solvent and sorbent material are preferably in 3～12 hours duration of contact.
Above-mentioned air regenesis tolerance is preferably in 1.8～3.0NM
3/ hrKg molecular sieve.
Require dew point to be preferably lower than-40 ℃ at described air moisture content.
The present invention adopts physical adsorption, the desorption method that periodical operation is carried out in a tower, and technical process is simple, and is easy to operate, the dehydration degree of depth is low, can make the dehydration of organic solvent degree of depth to 500ppm, the best can be to 5ppm, and minor amount of water removes in the suitable multiple organic solvent.
Below by embodiment in detail the present invention is described in detail.
Accompanying drawing 1 dewatering process equipment flowsheet.
Embodiment 1
Equipment used is seen accompanying drawing 1, mainly constitute by air compressor (1), air-heating furnace (2), head tank (3), dehydration tower (4), product jar (5) five parts, dehydration tower (4) bottom joins with head tank (3) by valve C (6), passes through valve B (9) emptying downwards simultaneously; Its top joins with product jar (5) by valve D (7), passes through valve A (8) simultaneously and links to each other with air compressor (1) with air-heating furnace (2).Air-heating furnace (2) is a jetting type heat pipe electrical heater, and 200～500 ℃ of outlet air temperatures are to satisfy the adsorbent reactivation processing condition.
The alcohol of 1% (V) water content is fed 4A molecular sieve (Dalian Chemistry and Physics Institute product) dehydration tower, and the granularity of adsorbent of molecular sieve is φ 15 to φ 30 orders; Dehydration tower internal diameter φ 110mm, high 3.0m, aspect ratio 27, be 5 hours the duration of contact of alcohol and sorbent material, treatment capacity is 100Kg/ days alcohol; Tower internal adsorption agent loading amount 20Kg, alcohol liquid air speed 0.2h
-1The water content of tower outlet alcohol is initially 105ppm, and water content rises to about 200ppm after 2 days, and sorbent material penetrates loading capacity and can reach 10% (wt) water.When the water content of alcohol surpassed 200ppm, molecular sieve needed regeneration.At first took out 2 hours with vacuum pump, used the air purge dehydration tower again 2 hours, use 200～500 ℃ then, dew point is-40 ℃, air regenesis 4 hours, and adsorbent of molecular sieve is reusable.Regeneration tolerance is 2.4NM
3/ hour Kg molecular sieve.
Equipment is identical with embodiment 1, and 3A molecular sieve (Dalian Chemistry and Physics Institute product) dehydration tower is equipped with in the industrial organic solvent 1.1-ethylene dichloride feeding of water content 0.3% (wt), and the sorbent material granularity is φ 2～3mm; Dehydration tower internal diameter φ 300mm, high 3.5m, treatment capacity is 2 tons/day, and tower internal adsorption agent loading amount is 175Kg, and ethylene dichloride liquid air speed is 0.5h
-1Tower outlet ethylene dichloride water content is initially 40ppm, rises to 500ppm after 3 days, and sorbent material penetrates loading capacity 10% (wt) to water.When the ethylene dichloride water content surpasses 500ppm, stop dehydration operation, sorbent material needs regeneration.At first took out 3 hours with vacuum pump, used the air purge dehydration tower again 2 hours, then the air that feeds is slowly heated up, kept when being raised to 350 ℃ 4 hours, regeneration finishes.The regeneration air amount is 3.0M
3/ hour Kg molecular sieve.
Claims (7)
1. the removing process of minor amount of water in the organic solvent is characterized in that operating process is as follows:
(1) water smoking
Make organic solvent with the void tower linear speed of 0.5～20cm/min by the sorbent material in the fixed bed packing tower, the aspect ratio 5～30 of tower, organic solvent fully contacts with sorbent material, 1～24 hour duration of contact, the initial water content of organic solvent should be less than 1%;
(2) purge stages of residual solvent in the tower
When sorbent material suction when saturated, storing liquid in tower is put only, vacuum desorption 1～5 hour was used for air purge 2～10 hours then, inflammable gas concentration is beyond limits of explosion in tower is worked off one's feeling vent one's spleen, air moisture content requirement dew point is lower than-20 ℃;
(3) the adsorbent reactivation stage
Be used for warm air sorbent material is regenerated under normal pressure, 200～500 ℃ of temperature, 2～24 hours time, air moisture content requires dew point to be lower than-20 ℃, regeneration tolerance 0.8～3.0NM
3/ hrKg molecular sieve;
(4) sorbent material temperature-fall period
Be used for freezing air temperature in the tower is reduced to normal temperature, air moisture content requires dew point to be lower than-20 ℃;
Above-mentioned steps repeats.
2. according to the removing process of minor amount of water in the described organic solvent of claim 1, it is characterized in that: organic solvent comprises aromatic hydrocarbons, alkanes, alcohols, amides, alkyl halide class; Sorbent material comprises A type, X type, Y type, mordenite type, ZSM type, MCM series molecular sieve.
3. according to the removing process of minor amount of water in claim 1, the 2 described organic solvents, it is characterized in that: tower aspect ratio 10～15, organic solvent and 3～12 hours duration of contact of sorbent material.
4. according to the removing process of minor amount of water in claim 1, the 2 described organic solvents, it is characterized in that: air regenesis tolerance 0.8～3.0NM
3/ hrKg molecular sieve.
5. according to the removing process of minor amount of water in claim 1, the 2 described organic solvents, it is characterized in that: air moisture content requires dew point to be lower than-40 ℃.
6. an equipment that is exclusively used in minor amount of water removing process in the described organic solvent of claim 1 mainly is made of air compressor (1), air-heating furnace (2), head tank (3), dehydration tower (4), product jar (5) five parts, it is characterized in that:
Dehydration tower (4) bottom joins with head tank (3) by valve C (6), passes through valve B (9) emptying downwards simultaneously; Its top joins with product jar (5) by valve D (7), passes through valve A (8) simultaneously and links to each other with air compressor (1) with air-heating furnace (2).
7. remove equipment according to minor amount of water in the described organic solvent of claim 6, it is characterized in that: air-heating furnace (2) is a jetting type heat pipe electrical heater, 200～500 ℃ of outlet air temperatures.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97126199 CN1117139C (en) | 1997-12-31 | 1997-12-31 | Dewatering tech. for microwater in organic solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97126199 CN1117139C (en) | 1997-12-31 | 1997-12-31 | Dewatering tech. for microwater in organic solvent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1221775A CN1221775A (en) | 1999-07-07 |
| CN1117139C true CN1117139C (en) | 2003-08-06 |
Family
ID=5177596
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97126199 Expired - Fee Related CN1117139C (en) | 1997-12-31 | 1997-12-31 | Dewatering tech. for microwater in organic solvent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1117139C (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008152351A1 (en) * | 2007-06-15 | 2008-12-18 | Bp Chemicals Limited | A method for the online analysis of a vapour phase process stream |
| CN103170160B (en) * | 2013-04-09 | 2015-01-07 | 六九硅业有限公司 | Water removal method by utilizing mixed solvent of methylbenzene and 1,2-dimethoxyethane |
| CN103933934B (en) * | 2014-05-07 | 2016-03-23 | 南京工业大学 | Adsorbent for removing trace moisture in gas and preparation method thereof |
| CN105080181B (en) * | 2014-05-20 | 2017-08-22 | 中石化广州工程有限公司 | A kind of method of C-4-fraction molecular sieve dehydration |
| CN105087048B (en) * | 2014-05-20 | 2017-06-20 | 中石化广州工程有限公司 | A kind of method of heavy naphtha molecular sieve dehydration |
| CN105732378B (en) * | 2014-12-08 | 2018-09-07 | 厦门伟捷化工工程有限公司 | A kind of method that organic-aqueous mixture carries out dehydration purification |
| CN104771933A (en) * | 2015-04-02 | 2015-07-15 | 周建伟 | Lubricating oil vacuum microwave water removing device |
| CN104877705A (en) * | 2015-06-01 | 2015-09-02 | 四川天采科技有限责任公司 | Method for normal-temperature adsorption dewatering of liquid phase of gasoline |
| CN112707838B (en) * | 2019-10-25 | 2022-12-09 | 中国石油化工股份有限公司 | Method for recovering N, N-dimethylacetamide |
| CN112479797B (en) * | 2020-11-30 | 2023-03-07 | 安徽泽升科技有限公司 | Preparation method of ultra-dry organic solvent |
-
1997
- 1997-12-31 CN CN 97126199 patent/CN1117139C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1221775A (en) | 1999-07-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA1149308A (en) | Process and apparatus for recovering hydrocarbons from air-hydrocarbon vapor mixtures | |
| CN1117139C (en) | Dewatering tech. for microwater in organic solvent | |
| JP2967871B2 (en) | Carbon dioxide and water adsorption method and adsorbent | |
| US5141724A (en) | Mercury removal from gaseous hydrocarbons | |
| EP1931612B1 (en) | Process and apparatus for the purification of methane rich gas streams | |
| CA2615439C (en) | Method of purifying hydrocarbons and regeneration of adsorbents used therein | |
| JP3537581B2 (en) | Mercury adsorbent | |
| US5447701A (en) | Gas purification method | |
| US5354357A (en) | Removal of mercury from process streams | |
| KR20080045178A (en) | Method and system for purifying a gas | |
| CN101342439A (en) | Hydrocarbons recovery method | |
| JP3569017B2 (en) | Method and apparatus for producing high-purity liquid nitrogen | |
| EP0678056A4 (en) | A packed bed and process for removal of residual mercury from gaseous hydrocarbons. | |
| CN1683249A (en) | Ingredient and process for producing copper (i) chloride, adsorbent and adsorbing method for reductive gas each with the use of copper (i) chloride, and recovering method of carbon monoxide gas | |
| US5271760A (en) | Recovery of liquid mercury from process streams | |
| US5190908A (en) | Racked bed for removal of residual mercury from gaseous hydrocarbons | |
| RU2241524C1 (en) | Method and apparatus for integrated purification of gases | |
| CN101370564A (en) | System and method for purifying a gas | |
| JPH01236941A (en) | Gaseous ammonia adsorbent | |
| KR20240023427A (en) | Ammonia Decomposition for Green Hydrogen | |
| CN101262924A (en) | Method and system for purifying a gas | |
| JPH0852304A (en) | Method of drying gaseous or liquid mixture using adsorbing device composed of alumina and molecular sieve | |
| JPH07284623A (en) | Method for treating and recovering concentrated gaseous hydrocarbon contained in discharged gas | |
| CN102949984A (en) | Macro-porous adsorption resin regeneration method | |
| JPH08281004A (en) | Device for removing lubricant in liquefied gas |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |